CN110106356A - A kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine - Google Patents
A kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine Download PDFInfo
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- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
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Abstract
The present invention relates to a kind of methods of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine.The present invention selects suitable powder-type titanium system ion-exchanger, first exchanger is effectively activated, after salt lake bittern to be adjusted to certain basicity again, by being filtered to remove the mechanical admixtures such as sediment silt, by after activation ion-exchanger and brine mixed in ion exchange pond, exchange reaction for a period of time after, ion-exchanger and salt lake bittern are separated by solid-liquid separation, ion-exchanger after separation carries out de- lithium processing with acid solution, rich lithium solution and regenerated ion-exchanger can be obtained, can be used for producing lithium carbonate and lithium hydroxide after rich lithium solution removal of impurities.This method apparatus and process process is simple, and the lithium ion adsorption capacity of ion-exchanger is high, the high long service life of selectivity.
Description
Technical field
The present invention relates to a kind of methods of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine, more particularly, to benefit
Method with a kind of titanium system powder-type ion-exchanger of highly selective high capacity, for separating Lithium from Salt Lake Brine ion.
Background technique
Lithium has extremely strong electro-chemical activity as the smallest metallic element of atomic weight, and chemical property is also extremely active.Cause
This, lithium can be reacted with generating with other materials for very comfortable, formed various alloys, be widely used in various fields.Lithium is answered
With mainly may be summarized to be new energy, new material and medical three big fields, mainly include battery, aerospace, nuclear fusion power plants,
Multiple subdivision fields such as metallurgy, ceramics, glass, lubricating grease, medicine.
According to the statistics of USGS, it is mainly salt lake bittern lithium resource that whole world lithium resource, which is constituted, at present, and reserves account for global total
The 72.31% of amount, the lithium resource of ore class occupy second, and the 20.26% of Zhan Quanqiu lithium resource reserves, it is in addition to this, remaining
Lithium ore resources mainly contain in oil gas field and terrestrial heat resources, the reserves of these resources account for about the whole world 7.43%.At present
The lithium carbonate raw material of worldwide production has 70% from salt lake bittern, only 30% comes from ore.And to propose lithium ratio lower for China's brine,
Ore proposes lithium accounting and is up to 80%.The saline lake lithium resource reserves in China account for the 64.81% of gross reserves, but due to China overwhelming majority
Salt lake resources are distributed in Qinghai-Tibet ecologically fragile area, and the exploitation of lithium resource is influenced by environment and technical barrier restricts.
Different salt lakes correspond to different lithium enrichments and propose lithium technique.Lithium in salt lake is typically all after producing sodium, potassium
It is extracted in remaining old halogen, old halogen, which carries out extracting lithium ion after pervaporation, demagging, concentration after lithium enrichment again, produces carbonic acid
Lithium.Tibetan Salt Lakes quality is preferable, but mining environment is undesirable；Qinghai Salt Lake can still be developed at present, but high Mg/Li ratio causes to mention lithium
Difficulty is big, compares overseas salt lake, needs additionally to carry out lithium enriching step, and salt lake corresponds to different lithiums due to bittern concentration difference
Enrichment proposes lithium technique.The salt lake bittern extractive technique used in the world at present mainly has the precipitation method, calcining leaching method, solvent extraction
Method, absorption method, electroosmose process etc..
The precipitation method are also known as solar pond method, are usually used in the higher salt pond of lithium concentration.The evaporation of old halogen is shone, the rich lithium of concentration is made
Brine removes boron and calcium ions and magnesium ions using acidification or extracting process, obtains the higher brine containing lithium.Soda ash precipitating reagent is added later
Lithium is separated with other salts.This method is more demanding to salt lake saline, and overall recovery is lower, and by solar evaporation by weather shadow
Sound is larger, and production capacity expansion is more difficult.
Calcining leaching method is will to mention the bittern evaporation after boron water is gone to obtain four aqueous magnesium chlorides, magnesia is obtained after calcining, so
Afterwards plus solution is concentrated by evaporation to being 2% or so containing Li, is added with the impurity such as milk of lime and soda ash removing calcium, magnesium by water extraction lithium
Soda ash is settled out lithium carbonate.Calcination method is conducive to comprehensively utilize the resources such as lithium magnesium, and consumption of raw materials is few, but the extraction of magnesium answers process
Miscellaneous, equipment seriously corroded, the water for needing to evaporate is larger, energy consumption is big, there are problems that environmental pollution, tight in current environmental protection
Under the supervision environment of control, biggish environmentally friendly risk is faced.
Solvent extraction is that after first carrying out old halogen to remove boron, FeCl is added3Solution forms LiFeCl4, use tributyl phosphate
(TBP)-kerosene extraction system is by LiFeCl4It is extracted into organic phase, becomes LiFeCl4The extracted species of+2TBP, are used after acid elution
Hydrochloric acid back extraction, then through processes such as evaporation and concentration, roasting, leaching, removal impurity, anhydrous lithium chloride can be obtained, be eventually adding carbonic acid
Sodium generates lithium carbonate.The method advantage is to be suitble to extract acid lithium salt from relatively salt lake brine with high magnesium-lithium ratio, but extracting
Brine amount to be treated is big in technique, larger to the corrosivity of equipment, there are problems that the molten damage of extractant, since waste liquid is organic
Object too high levels can cause very big pollution to salt lake, and extraction is unable to reach industry under higher and higher environmental protection standard and wants
It asks.
Electroosmose process is that salt lake bittern by one or more levels electric dialyzator, is utilized monovalent cation selectivity ion
Exchange membrane and univalent anion selectivity exchange membrane are recycled (continous way, continuous part circulating or batch cycles formula) technique
Lithium is concentrated, soda ash is added and is settled out lithium carbonate.But its technique requires to be the opposite general salt content of light brine lower than 100 grams per liters
Raw material, otherwise will cause that separating effect is bad, and cost significantly increases, which is that setting is simple, easy to operate, not dirty
Environment is contaminated, but separative efficiency is not high, filter membrane service life is shorter, and amberplex is not suitable for carbonic acid alkalinity brine.
Absorption method is selected first to the selective adsorbent of lithium, the lithium ion in salt lake bittern is adsorbed, then again
Lithium ion is eluted, the separation of lithium ion Yu other ions is reached, is convenient for subsequent handling trans-utilization.The key of the technique
It is lithium adsorbent, it is desirable that adsorbent can exclude the alkali metal largely coexisted in brine, the interference of alkaline-earth metal ions, and selectivity is inhaled
Lithium ion in attached brine, and require have adsorption capacity height, intensity high.But the adsorbent in currently available technology, which has absorption, to be held
Low, poor selectivity is measured, recycling rate is low, the technical problems such as equipment cost height.
Summary of the invention
It is high that the object of the present invention is to provide a kind of lithium ion adsorption capacities, and selectivity is high, powder-type titanium with long service life
It is ion-exchanger, the method for separating Lithium from Salt Lake Brine.
The method of the present invention includes the following steps:
The activation of titanium system ion-exchanger:
A. a certain amount of powder-type titanium system ion-exchanger is taken, ion water making is spent into 200~600g/L slurry, is reacting
40~75 DEG C are heated in tank；
B. it is slowly added to acid solution under stirring, terminal point control pH value is added dropwise 1.5~4.5, cures 2~8 hours
After be separated by solid-liquid separation；
C. repeat the above steps a and b, until Li content accounts for TiO in ion-exchanger2Content is less than 1.5%；
Separate the lithium in salt lake bittern:
D. the basicity of salt lake bittern is adjusted using alkaline matter；
E. it after brine being filtered to remove the mechanical admixtures such as sediment silt, squeezes into ion exchange pond；
F. it after the ion-exchanger after activation step (c) obtained is dispersed with brine slurrying, squeezes into ion exchange pond,
Using lasting aeration or mechanical stirring device, ion-exchanger is uniformly dispersed in brine and forms mixed slurry, prevents it
It settles；
G. after the completion of ion exchange, mixed slurry is separated by solid-liquid separation to obtain filter cake, filter cake is washed with deionized；
H. it by the filter cake deionized water after washing, after 200~600g/L slurry is made, is sent into reactor tank, and heat
To 40~75 DEG C；
I. acid solution is slowly added under stirring, control pH value 1.5~4.5, consolidated after 2~8 hours by curing
Liquid separation, obtains rich lithium solution and regenerated Lithium.
Wherein, the powder-type titanium system ion-exchanger in step a, molecular formula is a kind of Li(1.8X~2.2X)
TiXO(2.8X~3.2X)The compound of structural type, powder diameter 100nm≤D50≤100μm。
In step a, the activation temperature of ion-exchanger is at 45~75 DEG C.
In step b, the acid in the acid solution is one or more of hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, acetic acid, oxalic acid
Mixing.The final pH value control of the activation of ion-exchanger slurry is 2~4, more preferably 4.
In step c, the judgment criteria that ion-exchanger activation is completed is that Li content accounts for TiO in ion-exchanger2Content
0.01%~1%.
In step d, the alkaline matter be comprising alkali metal hydroxide, alkali carbonate, quick lime, white lime and
The mixing of one or more of ammonium hydroxide.The basicity for adjusting brine is total alkalinity.It is adjusted according to lithium concentration in brine
Section, numerical value should be controlled in 1~1.5 times of C(Li+), it is ensured that there is the H that in enough substances and ion exchange releases in brine+。
In step e, the filter method includes: sand filtration, plate-frame filtering or filter cartridge type filter filtering, brine after filtering
Turbidity answers≤5JTU.
In step g, ion exchange completes to refer to that the ion concentration in brine no longer declines or lithium ion is inhaled completely
It is attached；Washing terminal is to wash out water conductivity≤500 μ s/cm, preferably wash-off water conductivity≤100 μ s/cm.
In step h, the desorption temperature of ion-exchanger is 45~70 DEG C.
In step i, the acid in the acid solution of addition is one of hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, acetic acid, oxalic acid or several
The mixing of kind.The desorption terminal of ion-exchanger is to control the pH value of slurry 2~4, more preferably 4.
When salt lake bittern is calcareous type salt lake bittern, without progress step d.
The present invention compared with the prior art, have the following advantages that and the utility model has the advantages that
(1) the present invention provides a kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine, inventors
By concentrating on studies for many years, discovery, can be directly in office by the application activating process treated titanium system ion-exchanger
Carry out efficient ion exchange in the reactor tank or reaction tank of meaning, and the prior art must use adsorption column or ion exchange tower into
Row mentions lithium, greatly reduces the efficiency of ion exchange, and equipment operation is stringent, at high cost；Apparatus and process of the invention is simple,
It is easy to operate, the cost of industrial application is reduced, treatment effeciency is improved.
(2) prior art needs are made ion-exchanger adding assistant tabletting at ion sieve, or with organic and inorganic binder
It is filled after grain.Binder wraps exchanger surface, and the contact area of exchanger and brine is greatly reduced, and seriously affects friendship
Throw-over degree.With the increase of cycle-index, dusting, failure can also occur for material.This method does not need to be granulated, and because ion exchange
The dusty material of agent itself is directly contacted with brine, and contact area is big, and reaction efficiency is high, and the reaction time is shorter, and material will not
The influence for thering is dusting to fail.
(3) in contrast to manganese systems ion-exchanger and aluminium system ion-exchanger, can all have during de- lithium considerable amount of molten
Damage problem, and adsorbance is gradually declining.The titanium system ion-exchanger that the present invention activates, without molten damage, and is inhaled during de- lithium
The although curved variation of attached amount, but there is no decline for total adsorbance, so that and ion-exchanger has longer service life.
(4) in contrast to manganese systems ion-exchanger and aluminium system ion-exchanger, the titanium system ion-exchanger that the present invention activates has
There are higher adsorption capacity, and lithium concentration > 10g/L in the rich lithium solution after de- lithium.
Detailed description of the invention
Attached drawing 1 is to mention lithium by 10 circulations, lithium ion content curve graph in ion-exchanger.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the present invention is further illustrated, but protection scope of the present invention is not
It is limited to this.
Embodiment 1
The slurry for taking a certain amount of powder-type titanium system ion-exchanger to spend ion water making into 200g/L adds in reactor tank
Heat is slowly added to acid solution to 40 DEG C in stirring, terminal PH to 4.5 is added dropwise, and curing is filtered after 8 hours, repetitive operation to ion
Li content accounts for TiO in exchanger2The 1% of content；It is 1 times with the basicity that alkaline matter adjusts salt lake bitternAfter filtering
Brine turbidity is 5JTU, and filtered brine is squeezed into ion exchange pond；By the filtered brine slurrying of ion-exchanger, divide
Ion exchange pond is also squeezed into after dissipating uniformly, after being stirred to react completely, after slurries filtration is separated by solid-liquid separation, filter is washed with deionized
Cake to washing water conductivity is 300 μ s/cm；Filter cake spends ion water making into the slurry of 300g/L, and 40 are heated in reactor tank
DEG C, it is slowly added to acid solution in stirring, terminal PH to 4.5 is added dropwise, curing is filtered after 8 hours, obtains rich lithium solution and regenerated
Ion-exchanger, lithium concentration is 10.62g/L in rich lithium solution.
Embodiment 2
The slurry for taking a certain amount of powder-type titanium system ion-exchanger to spend ion water making into 600g/L adds in reactor tank
Heat is slowly added to acid solution to 75 DEG C in stirring, terminal PH to 1.5 is added dropwise, and curing is filtered after 5 hours, repetitive operation to ion
Li content accounts for TiO in exchanger2The 0.5% of content；It is 1.25 times with the basicity that alkaline matter adjusts salt lake bitternIt crosses
Brine turbidity is 2JTU after filter, and filtered brine is squeezed into ion exchange pond；By the filtered making from brine of ion-exchanger
Slurry, also squeezes into ion exchange pond after being uniformly dispersed, after being stirred to react completely, after slurries filtration is separated by solid-liquid separation, use deionized water
Washing filter cake to washing water conductivity is 200 μ s/cm；Filter cake spends ion water making into the slurry of 600g/L, adds in reactor tank
Heat is slowly added to acid solution to 75 DEG C in stirring, terminal PH to 1.5 is added dropwise, and curing is filtered after 2 hours, obtain rich lithium solution and
Regenerated ion-exchanger, lithium concentration is 11.19g/L in rich lithium solution.
Embodiment 3
The slurry for taking a certain amount of powder-type titanium system ion-exchanger to spend ion water making into 400g/L adds in reactor tank
Heat is slowly added to acid solution to 60 DEG C in stirring, terminal PH to 4.0 is added dropwise, and curing is filtered after 2 hours, repetitive operation to ion
Li content accounts for TiO in exchanger2The 0.01% of content；It is 1.5 times with the basicity that alkaline matter adjusts salt lake bitternIt crosses
Brine turbidity is 3JTU after filter, and filtered brine is squeezed into ion exchange pond；By the filtered making from brine of ion-exchanger
Slurry, also squeezes into ion exchange pond after being uniformly dispersed, after being stirred to react completely, after slurries filtration is separated by solid-liquid separation, use deionized water
Washing filter cake to washing water conductivity is 100 μ s/cm；Filter cake spends ion water making into the slurry of 400g/L, adds in reactor tank
Heat is slowly added to acid solution to 60 DEG C in stirring, terminal PH to 4.0 is added dropwise, and curing is filtered after 5 hours, obtain rich lithium solution and
Regenerated ion-exchanger, lithium concentration is 12.37g/L in rich lithium solution.
Partial results during embodiment are detected, wherein ion concentration is Agilent ICP-OES testing result.
Table 1: the part detection data of embodiment 1
Table 2: the part detection data of embodiment 2
Table 3: the part detection data of embodiment 3
The invention is not limited to specific embodiments above-mentioned.The present invention, which expands to, any in the present specification to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.It cannot be with
This is limited the scope of implementation of the present invention, therefore the displacement of its equivalent assemblies, or is equally become according to made by the invention patent protection scope
Change and modify, should still belong to the scope that claims of the present invention is covered.
Claims (10)
1. a kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine, which comprises the following steps:
(1) activation of titanium system ion-exchanger:
A, a certain amount of powder-type titanium system ion-exchanger is taken, spends ion water making at 200~600g/L slurry, in reactor tank
It is heated to 40~75 DEG C；
B, it is slowly added to acid solution under stirring, terminal point control pH value is added dropwise 1.5~4.5, curing 2~8 hours laggard
Row is separated by solid-liquid separation；
C, repeat the above steps a and b, until Li content accounts for TiO in ion-exchanger2Content is less than 1.5%；
(2) lithium in salt lake bittern is separated:
D, the basicity of salt lake bittern is adjusted using alkaline matter；
E, it by after brine impurity screening, squeezes into ion exchange pond；
F, it after the ion-exchanger after the activation for obtaining step (c) is dispersed with brine slurrying, squeezes into ion exchange pond, utilizes
Lasting aeration or mechanical stirring device, ion-exchanger is uniformly dispersed in brine and forms mixed slurry, prevents its generation
Sedimentation；
G, after the completion of ion exchange, mixed slurry is separated by solid-liquid separation to obtain filter cake, filter cake is washed with deionized；
H, it by the filter cake deionized water after washing, after 200~600g/L slurry is made, is sent into reactor tank, and be heated to 40
~75 DEG C；
I, acid solution is slowly added under stirring, control pH value carries out solid-liquid point after 1.5~4.5, curing 2~8 hours
From obtaining rich lithium solution and regenerated Lithium.
2. a kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine according to claim 1, special
Sign is, in step a, the powder-type titanium system ion-exchanger, molecular formula is a kind of Li(1.8X~2.2X)TiXO(2.8X~3.2X)
The compound of structural type, powder diameter 100nm≤D50≤100μm。
3. a kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine according to claim 1, special
Sign is, in step a, the activation temperature of ion-exchanger is at 45~75 DEG C.
4. a kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine according to claim 1, special
Sign is, in step b, the acid in the acid solution is one or more of hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, acetic acid, oxalic acid
Mixing.
5. a kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine according to claim 1, special
Sign is, in step b, the final pH value control of the activation of ion-exchanger slurry is 4.
6. a kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine according to claim 1, special
Sign is, in step c, the judgment criteria that ion-exchanger activation is completed is that Li content accounts for TiO in ion-exchanger2Content
0.01%~1%.
7. a kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine according to claim 1, special
Sign is, in step d, the alkaline matter be comprising alkali metal hydroxide, alkali carbonate, quick lime, white lime and
The mixing of one or more of ammonium hydroxide.
8. a kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine according to claim 1, special
Sign is, in step d, the basicity for adjusting brine is total alkalinity；It is adjusted according to lithium concentration in brine, numerical value is answered
Control is in 1~1.5 times of C(Li+), it is ensured that there is the H that in enough substances and ion exchange releases in brine+；And/or step e
In, the filter method includes: sand filtration, plate-frame filtering or filter cartridge type filter filtering, and brine turbidity answers≤5JTU after filtering；
And/or in step g, ion exchange completes to refer to that the ion concentration in brine no longer declines or lithium ion is adsorbed completely；
Washing terminal is to wash out water conductivity≤500 μ s/cm；And/or in step h, the desorption temperature of ion-exchanger is 45~70
℃；And/or in step i, acid in the acid solution of addition be one of hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, acetic acid, oxalic acid or
Several mixing.
9. a kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine according to claim 1, special
Sign is, in step i, the desorption terminal of ion-exchanger is to control the pH value of slurry 4.
10. a kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine according to claim 1, described
Salt lake bittern is calcareous type salt lake bittern, without progress step d.
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Cited By (2)
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| WO2021223014A1 (en) * | 2020-05-07 | 2021-11-11 | Prairie Lithium Corporation | Methods and systems for recovery of valuable target species from brine solutions |
| CN114086006A (en) * | 2021-11-22 | 2022-02-25 | 南京工业大学 | Lithium extraction process for coupling powdery lithium adsorbent with hollow fiber membrane |
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| CN105238927A (en) * | 2015-11-09 | 2016-01-13 | 华东理工大学 | Titanium-based lithium ion sieve adsorbent, precursor thereof, preparation methods and application |
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| JPH024442A (en) * | 1988-06-21 | 1990-01-09 | Agency Of Ind Science & Technol | High performance lithium adsorbent and its preparation |
| CN1491891A (en) * | 2003-09-12 | 2004-04-28 | 成都理工大学 | New process for synthesizing lithium ion separation material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2021223014A1 (en) * | 2020-05-07 | 2021-11-11 | Prairie Lithium Corporation | Methods and systems for recovery of valuable target species from brine solutions |
| US20210346822A1 (en) * | 2020-05-07 | 2021-11-11 | Prairie Lithium Corporation | Methods and systems for recovery of valuable target species from brine solutions |
| CN114086006A (en) * | 2021-11-22 | 2022-02-25 | 南京工业大学 | Lithium extraction process for coupling powdery lithium adsorbent with hollow fiber membrane |
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